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INETI-DMTP, LCM – Laboratório de Caracterização de Materiais, Estrada do Paço do Lumiar, 1649-038 Lisboa
teresa.ferraz@ineti.pt
ABSTRACT: his paper details the analysis carried out on two failed bolts to find out the reason for failure, using
macrofractography, optical metallography and scanning electron microscope (SEM) techniques. Usual measures to preventt
such failures are also referred. Similar fractures occurred at the head to shank transition of the bolts during fastening, orr
afterwards, while waiting for delivery. Since failure occurred in a region where foreseen stresses were quite below yield
strength and there was no evidence of mechanical deformation, embrittlement was suspected. SEM observation of the
fracture surface crack initiation region showed areas of intergranular crack propagation indicating brittleness, and higherr
magnification observation showed hydrogen embrittlement features. The bolts, which microstructure was typically that off
hardened and tempered steel, had been zinc electroplated and it is well known that hydrogen release concurs with zinc
deposition. Moreover, the diffusion and accumulation of the hydrogen in metals is favoured by cold working, as is the case
of the head to shank transition region.
RESUMO: Este artigo apresenta a análise efectuada em dois parafusos fracturados, com o objectivo de determinar as
causas da fractura, usando técnicas de macrofractografia, metalografia óptica e microscopia electrónica de varrimento.
Também são referidas as precauções habituais para evitar este tipo de falha. As fracturas, semelhantes entre si,
ocorreram na transição entre a cabeça e o corpo do parafuso, durante ou após a operação de aperto. Uma vez que as
fracturas apareceram numa região em que as tensões previstas estariam bastante abaixo da tensão de cedência e não se
observava deformação mecânica, a fragilização foi desde logo uma possível suspeita. A observação da superfície na
zona de iniciação da fractura, por microscopia electrónica de varrimento, revelou zonas de propagação intergranular de
fissuras, apontando para uma fragilização, sendo possível observar aspectos típicos de fragilização por hidrogénio a
ampliações mais elevadas. Os parafusos, cuja microestrutura correspondia à de um aço temperado e revenido, tinham
sofrido um tratamento superficial de zincagem. Sabe-se que, durante estes tratamentos, a libertação de hidrogénio
compete com a deposição do zinco e, além disso, a difusão e acumulação do hidrogénio nos metais é favorecida pela
deformação a frio, o que é precisamente o caso da zona de transição cabeça/corpo de um parafuso.
Palavras chave: Fragilização por hidrogénio, falha, aço, fractografia, microscopia electrónica de varrimento
However, when high strength steel fasteners are required, Hydrogen embrittlement is a well-known phenomenon in
such as ISO 898-1 grade 10.9 or higher, for which nominal which a metal is weakened by the incorporation of hydrogen
tensile strengths over 1000 MPa are specified, bolts are in or below its surface, e.g. during plating or etching.
made of quenched and tempered steel [2], and electroplating Hydrogen diffuses easily into the metal crystalline structure
presents a high risk of hydrogen embrittlement. It is well either as atoms or protons. Non-metallic inclusions such as
known that during zinc electroplating hydrogen release sulphides, as well as phosphorus, favour hydrogen
concurs with zinc deposition. Besides selecting plating adsorption, acting as catalysts. Grain boundaries and other
128 Ciência e Tecnologia dos Materiais, Vol. 20, n.º 1/2, 2008
Hydrogen embrittlement M. Teresa Ferraz and Manuela Oliveira
lattice defects are also regions where hydrogen diffuses and deformation) in the transition zone between head and
accumulates easily, hence preferential for hydrogen shank;
embrittlement to occur. Hydrogen diffusion is also easier in - there was no general oxidation and/or corrosion;
all regions where the crystalline structure may be distorted - fracture surfaces were quite smooth and normal to the
as a result of work hardening or cold deformation. The direction of the applied loads, except for the central part
accumulation of hydrogen restricts ductility and promotes corresponding to the end of fracture;
brittleness. - fractures seemed to have had its origin all around the
circular external bolt surface, where several initiating
Hardened and tempered steels need only a few p.p.m. of zones were observed.
hydrogen to cause embrittlement [3, 4].
The following tests were carried out:
Failure induced by hydrogen is favoured or caused by
applied stresses, even static or of low intensity, and is - Fractographic examination of both bolts fracture
often referred to as “delayed” or “retarded”, since it may surfaces at low magnifications (3 to 20 times) with an
not take place immediately after tensile stresses are optical stereomicroscope and also at higher
applied. This type of embrittlement is not detectable by magnification with a SEM (20 to 10000 times) after
hardness determinations, but tensile tests will show ultrasonic cleaning in an ethylic alcohol bath.
considerable reduction of the expected tensile strength of - Metallographic examination by optical microscopy of
the material [5]. the fractured bolts microstructure on longitudinal
sections from the head and shank part nearest to the
This work presents a case study where premature fragile head taken through the bolt axis.
- Rockwell C hardness determinations on a cross section
failure of several bolts occurred, during assembly of
components, or afterwards while waiting for delivery of the shank.
(delayed failure), at low stresses, quite below the specified
proof stress.
3. RESULTS
3.1. FRACTOGRAPHY
2. FAILURE ANALYSIS
Observations at low magnification (Fig. 2) showed that:
The fractures occurred at the head to shank transition of
several steel fasteners used to fix an engine to its base. The - Fracture characteristics were similar in both bolts
following items and information were provided for failure indicating that failure must have occurred by the same
analysis: causes;
- the fractures were almost parallel to the cross section,
- Photographs of a component with a fractured bolt inside and occurred with no evidence of deformation or
and of two fractured bolts (Fig. 1); distortion near the origin;
- two fractured bolts (head and shank); - the fracture surfaces were nearly flat with several crack
- bolts were supposed to be class 10.9 (ISO 898-1) and initiation zones all around the external bolt surface;
zinc electroplated. - origins were located at slightly different levels and after
a short propagation cracks joined together in a common
front;
- the fracture surface area corresponding to this first stage
of propagation showed the smoothest surface on fig. 2
b) and 2 c);
- cracks continued to propagate towards the centre, and
fracture surfaces became rougher;
- final rupture occurred by overload shear and showed a
change in crack propagation direction towards the top
of the bolt head;
- both fractures occurred almost instantaneously after
cracking initiation due to the applied stresses.
Ciência e Tecnologia dos Materiais, Vol. 20, n.º 1/2, 2008 129
M. Teresa Ferraz and Manuela Oliveira Hydrogen embrittlement
a)
Init
a)
b)
b)
Fig. 3. SEM observation of one of the bolts fracture
surfaces: a) overall view of initiation zones near shank
external surface; b) detail from marked area, fracture
propagation partially intercrystalline and transcrystalline,
intergranular zones showing intercrystalline subsidiary
cracking, micro-pores and ductile hair lines at the former
c) austenite grain boundaries.
Fig. 2. Fractured bolt: a) General side view of facture
surface, shank side; b) details of fracture initiation zones at
head-shank transition surface, shank side; c) details of
fracture initiation zones at head-shank transition surface,
head side.
130 Ciência e Tecnologia dos Materiais, Vol. 20, n.º 1/2, 2008
Hydrogen embrittlement M. Teresa Ferraz and Manuela Oliveira
a)
c)
Ciência e Tecnologia dos Materiais, Vol. 20, n.º 1/2, 2008 131
M. Teresa Ferraz and Manuela Oliveira Hydrogen embrittlement
The flatness of fracture surfaces, the serial failures and the Zn2+ + 2e- = Zn0 (1)
fact that failure process took place in a region where, when 2 H+ + 2e- = H2 (2)
in service, expected tensile stresses are considerably lower
(at least twice to three times lower) than those expected after Therefore, the electrolytic process must be controlled,
fastening in the threaded shank zone at the first thread inside namely high efficiency procedures must be used, current
the nut, pointed out to a manufacture or material defect or to intensity and bath impurities controlled and good agitation
an embrittlement phenomenon as causes for failure. provided in order to liberate the hydrogen bubbles formed
over the cathode surface. The control may not always be
The microstructure observed corresponded to hardened and efficient in order to prevent hydrogen from concentrating in
tempered steel, without detectable preferential carbide microstructure defects and some hydrogen may be
precipitation along previous austenite grain boundaries, so inevitably present.
carbide embrittlement was excluded. Surface
decarburization was not detected either. The solubility of hydrogen decreases with temperature and
hydrogen accumulated in lattice defects may precipitate in
Inclusion content of the steel was far below the maximum gaseous form, originating a pressure high enough to produce
limits accepted for this kind off application. Forging defects, small cracks. This can however be avoided by a post plating
cracks or other discontinuities, that could have acted as stress baking treatment to remove hydrogen prior to service [3,4].
concentrators or raisers were also not observed. Finally, there Zinc electroplated components must undergo the treatment
was not oxidation of the fracture surface, or crack branching at temperatures around 200oC, for several hours and
along grain boundaries, which would indicate quenching immediately or shortly after plating.
cracking or a stress corrosion crack process.
Internal hydrogen embrittlement has been known for years,
The observation of the fracture surfaces carried out in the but is far away from being banished or even controlled.
SEM showed that, starting at the external surface, crack Some components may require longer baking times due to
132 Ciência e Tecnologia dos Materiais, Vol. 20, n.º 1/2, 2008
Hydrogen embrittlement M. Teresa Ferraz and Manuela Oliveira
more gas evolution during plating or to thicker and less [2] ISO 898-1:1999, “Mechanical properties of fasteners
permeable coatings. To prevent risk of failure due to made of carbon steel and alloy steel – Part 1: Bolts,
improper baking after electroplating, standardized tests on screws and studs.
samples may be conducted [7,8]. Another alternative is to
choose a coating procedure without hydrogen embrittlement [3] Kim, C.D., “Hydrogen-Damage Failures”, in “Metals
risk. Handbook”, Ninth Edition, Vol 11, 245-251, American
Society for Metals, Metals Park, Ohio, U.S.A. (1986).
Ciência e Tecnologia dos Materiais, Vol. 20, n.º 1/2, 2008 133